Inorganic experiments

Renew your inorganic chemistry lab course. This completely revised and enlarged second edition of the classic now includes over 20 new experiments reflecting modern research, with many of the compounds only having very recently been described. The book offers detailed descriptions of more than 80 experiments, ranging from undergraduate to graduate level, covering organometallic, main group, solid state and coordination chemistry. Almost all reaction types, laboratory techniques and classes of compounds which constitute current curricula are exemplarily represented. University teachers from all over the world have contributed experiments, each of which has been thoroughly tested. Special safety instructions are provided in each case, with highly hazardous substances substituted by less harmful ones wherever possible. The products are characterized by modern spectroscopic techniques and the book also includes exercises, questions and hints for further reading. A whole new set of experiments considers new knowledge gained by science education research: Discovery-oriented open-end experiments that resemble real research, allowing both teachers and students a more fascinating and efficient approach to standard courses in inorganic chemistry, already training the group-oriented approach to research carried out in academic and industrial settings.

• Preface
• 1 Introduction p. 1
• 1.1 Introduction p. 3
• 1.2 Introduction to Discovery Oriented/Group Learning Laboratory Experiences p. 4 Allen D. Hunter
• 2 Introductory Experiments p. 7
• 2.1 Preparation and Investigation of Some Coordination Compounds p. 9 Roderick D. Cannon and Manfred Bochmann
• 2.2 Gravimetric Analysis of Hexaammine Nickel(II) Tetrafluoroborate, [Ni(NH subscript 3) subscript 6 (BF subscript 4) subscript 2] p. 12 Roderick D. Cannon and Manfred Bochmann
• 2.3 Analysis of an Iron(III) Oxalate Complex p. 17 Roderick D. Cannon and Manfred Bochmann
• 2.4 Characterisation of a Copper Oxalate Complex K[subscript a]Cu[subscript b](C[subscript 2]O[subscript 4])[subscript c]-dH[subscript 2]O p. 22 Andrew W. G. Platt
• 2.5 Vanadium Alum: An Experiment in Electrosynthesis p. 24 David T. Richens
• 2.6 Ammonium Dichromate, Chromium(III) Oxide, Potassium Chromate and Potassium Tetraperoxochromate (V) p. 27 Antonin Ruzicka and Zdirad Zak
• 2.7 Linkage Isomerism: An Infra-Red Study p. 31 David T. Richens and Christopher Glidewell
• 2.8 Preparation and Complexation of Tris(3,5-dimethylpyrazoyl)hydroborate p. 33 Manfred Bochmann
• 2.9 Tetraiodotin(IV) and its Triphenylphosphine Complex p. 36 J. Derek Woollins
• 2.10 Silicon Oxygen Compounds and Siloxane Polymers p. 38 Paul D. Lickiss
• 2.11 Preparation and NMR Identification of Two Phosphorus Esters p. 42 Christopher Glidewell
• 2.12 The Preparation of Potassium Peroxodisulphate, K[subscript 2]S[subscript 2]O[subscript 8] p. 44 Zdirad Zak and Antonin Ruzicka
• 2.13 K[subscript 2]ON (SO[subscript 3])[subscript 2] (Fremy's Salt) and [Ph subscript 3 PCH subscript 2 C subscript 6 H subscript 4 CH subscript 2 PPh subscript 3 ON(SO subscript 3) subscript 2] p. 47 David M. L. Goodgame
• 2.14 Polyiodides, Me[subscript 4]NI[subscript x] p. 49 Andrew W. G. Platt
• 2.15 Interhalogen Compounds p. 51 Ivan P. Parkin
• 2.16 Synthesis and Infrared Spectroscopic Characterisation of Boranes and Germanes p. 56 Ivan P. Parkin
• 2.17 Deduction of the Coordination Mode of BH[subscript 4] in Bis(triphenylphosphine) Copper(I) Borohydride (Ph[subscript 3]P)[subscript 2]CuBH[subscript 4] p. 61 Andrew W. G. Platt
• 2.18 Synthesis and Characterisation of a Metal Hydride Complex p. 64 Andrew W. G. Platt
• 2.19 Preparation and Identification of a Copper(I) Complex p. 66 Andrew W. G. Platt
• 2.20 Synthesis of [NH subscript 4] [BF subscript 4] and Synthesis and Titrimetric Analysis of [Zn(NH subscript 3) subscript 4] [BF subscript 4 subscript 2] p. 68 Michael A. Beckett
• 2.21 Iron(II) and Lead(II) Formates p. 71 Francisco J. Arnaiz and Maria R. Pedrosa and Rafael Aguado
• 2.22 Preparation of Copper(I) Iodide p. 75 F. J. Arnaiz and M. R. Pedrosa and S. Arnaiz
• 2.23 Discovery Research with Siloxane Chemistry p. 77 Allen D. Hunter
• 3 Intermediate Experiments p. 83
• 3.1 Ferrocene, ([eta superscript 5]-C[subscript 5]H[subscript 5])[subscript 2]Fe, and Its Derivatives p. 85 J. Derek Woollins
• 3.2 The Use of Organolithium Reagents in the Preparation of Ferrocene Derivatives p. 88 Ian R. Butler
• 3.3 Complexes of [Pi]-Bonding Arene Ligands p. 95 Andrew W. G. Platt
• 3.4 Organotin Chemistry p. 98 Kieran C. Molloy and Timothy T. Paget
• 3.5 Nickel Catalysed Cross-Coupling of Alkylmagnesium with Haloarene p. 105 G. Brent Young
• 3.6 Transition Metal Catalysis p. 109 Neil M. Boag
• 3.7 Transition Metal-Carbon Bonds in Chemistry and Biology p. 113 C. J. Jones
• 3.8 Cobalt Complexes of Dioxygen p. 124 David T. Richens and Christopher Glidewell
• 3.9 Preparation of Nitrosyl Complexes of Iron and Nickel p. 127 Andrew W. G. Platt and John F. Gibson
• 3.10 Preparation of an Iron Dinitrogen Complex p. 130 Andrew W. G. Platt
• 3.11 Nickel Dihalide Phosphine Complexes p. 132 Ivan P. Parkin
• 3.12 Influence of Ligand Field Tetragonality on the Ground-State Spin of Nickel(II) Complexes p. 136 David M. L. Goodgame
• 3.13 Preparation of Trans-PtHCl(PPh[subscript 3])[subscript 2] and Measurement of its [superscript 1]H, [superscript 31]P and [superscript 195]Pt NMR Spectra p. 139 William P. Griffith
• 3.14 Identification of Stereochemical (Geometrical) Isomers of [Mo(CO) subscript 4 (L) subscript 2] by Infra-Red Spectroscopy p. 143 Michael A. Beckett
• 3.15 Five Coordinate Complexes: [VO(acac) subscript 2] and [Cr(NH subscript 3) subscript 6] [CuCl subscript 5] p. 146 Christopher P. Morley
• 3.16 Metal Acetylacetonate Complexes: Preparation and Characterisation p. 149 Christopher Glidewell
• 3.17 Nickel(II) Complexes of Some Schiff Base Ligands p. 160 C. J. Jones
• 3.18 The Synthesis and Coordination Chemistry of Macrocyclic Complexes p. 167 Martin Schroder
• 3.19 Synthesis and Reactivity of Tertiary Phosphines p. 172 Neil M. Boag
• 3.20 Inorganic Heterocycles: Cyclophosphazenes p. 176 Josef Novosad and Milan Alberti
• 3.21 Inorganic (Carbon-Free) Chelate Rings: A Dithioimidodiphosphinato Ligand and Some of its Metal Complexes p. 179 Ionel Haiduc
• 3.22 Amidosulfuric Acid, Trisilveramidosulfate Monohydrate and SO[subscript 3] - N(CH[subscript 3])[subscript 3] Complexes p. 184 Antonin Ruzicka and Zdirad Zak
• 3.23 Four Methods for Analysing First Order Kinetics p. 188 Veronique Pimienta and Dominique Lavabre and Jean-Claude Micheau and Gaston Levy
• 3.24 Inorganic (Carbon-Free) Chelate Rings II: Asymmetrical Mixed-Donor P-N-P Ligand and its Palladium Complex p. 194 David J. Birdsall and Josef Novosad
• 3.25 [MoO subscript 2 Br subscript 2 (H subscript 2 O) subscript 2] - (diglyme) and [MoO subscript 2 Br subscript 2 (DMF) subscript 2] p. 199 Francisco J. Arnaiz and Maria R. Pedrosa and Rafael Aguado
• 3.26 Nitration of Cobalt(III)acetylacetonate p. 203 David J. Otway
• 3.27 [Co(dinosar)]Cl[subscript 3]: An Encapsulation Complex Prepared by a Template Reaction p. 205 David J. Otway
• 3.28 Anomalous Paramagnetism in Some Iron(III) Chelates Studied by the Evans NMR Method p. 208 David J Otway
• 3.29 Solid Sodium Amalgam p. 211 Allen D. Hunter
• 3.30 Discovery Research with Cyclopentadienyl Iron Carbonyl Chemistry p. 214 Allen D. Hunter
• 3.31 Discovery Research with Model One-Dimensional Organometallic Materials of Ni, Pd, and Pt p. 222 Allen D. Hunter
• 4 Advanced Experiments p. 227
• 4.1 Chlorotris(tert-butylimido)manganese(VII) p. 229 Andreas A. Danopoulos and Geoffrey Wilkinson
• 4.2 2,2':6',2"-Terpyridine Complexes and Metal Directed Reactivity p. 232 Edwin C. Constable
• 4.3 Electronic Characterisation of a Transition-Metal Complex Using Electrochemical UV/Vis and EPR Techniques p. 235 Lesley J. Yellowlees
• 4.4 The Synthesis of [eta superscript sigma]-Arenetricarbonyl Chromium(0) Complexes p. 238 David A. Widdowson
• 4.5 Migratory Insertion Reactions in Organo Transition-Metal Chemistry p. 241 Mark J. Winter
• 4.6 Organometallic Molybdenum Compounds p. 246 Manfred Bochmann and Paul Hammerton
• 4.7 The Preparation of rac-Ethylene-1,2-bis(1-indenyl)zirconium Dichloride and Dibenzyl Complexes p. 252 Manfred Bochmann and Simon J. Lancaster
• 4.8 Halfsandwich Carbonyl Vanadium Complexes p. 257 Max Herberhold and Matthias Schrepfermann
• 4.9 Covalent and Ionic Metallocene Hexafluoroarsenate Complexes p. 263 Inis C. Tornieporth-Oetting and Thomas M. Klapotke
• 4.10 Preparation of the Iron Tricarbonyl Complex of Methyl-2-Acetamidoacrylate p. 266 Simon R. Drake and M. Elena Lasterra-Sanchez and Susan E. Thomas
• 4.11 A Transition-Metal Alkylidyne Complex p. 268 Stephen Anderson and Darren Cook and Anthony F. Hill
• 4.12 Preparation of [Bu subscript 4 N] [B subscript 3 H subscript 8] and the Formation of RuH[B subscript 3 H subscript 8](CO)(PPh subscript 3)[subscript 2] p. 271 Anthony F. Hill and J. Derek Woollins
• 4.13 Vacuum Line Techniques: Preparation of SiF[subscript 4] and SiF[subscript 4](C[subscript 5]H[subscript 5]N)[subscript 2] p. 275 Dennis F. Evans and J. Derek Woollins
• 4.14 Preparation and Structure of the Acetyl Chloride-Antimony Pentachloride Complex p. 279 Peter N. Gates
• 4.15 Arsenium Cations: Carbene Analogues p. 282 Neil Burford and Trenton M. Parks
• 4.16 Preparation and Some Reactions of the Folded P[subscript 2]N[subscript 4]S[subscript 2] Ring p. 287 Tristram Chivers and Daniel D. Doxsee and Robert W. Hilts
• 4.17 Sulfur-Rich Homocycles and Heterocycles: Titanocene Pentasulfide Cyclo-Heptasulfur and 1,2,3,4,5,6,7-Heptathionane p. 291 Jorg Albertsen and Ralf Steudel
• 4.18 Reaction of Alkali Metal Polyselenides and Polytellurides with Group 6 Metal Carbonyls p. 295 Joseph W. Kolis
• 4.19 Sulphur-Nitrogen Heterocycles and [SNBr subscript 0.4 subscript x] Polymer p. 300 J. Derek Woollins
• 4.20 Chlorothionitrene and Cyclothiazeno Complexes of Tungsten p. 304 Kurt Dehnicke
• 4.21 Selenium-Nitrogen and Tellurium-Nitrogen Compounds p. 307 Herbert W. Roesky and Judith Gindl
• 4.22 Nitride Chlorides of Selenium(III) and Selenium(IV): Se[subscript 2]NCl[subscript 3] and Se[subscript 2]NCl[subscript 5] p. 311 Kurt Dehnicke
• 4.23 Structural, Electrical and Magnetic Properties of Perovskite Ceramics p. 315 Colin Greaves
• 4.24 Metal-containing Liquid Crystals. The Synthesis of trans-bis(4-Alkyl-4'-cyano-1,1'-biphenyl)dichloroplatinum(II) and Related Species--The Use of Melt Syntheses p. 321 Duncan W. Bruce
• 4.25 Magnetochemistry Experiments: Exchange Coupling in Copper(II)-Nickel(II) Bimetallic Complexes and Spin Transition in Iron Complexes p. 329 E. Coronado and J. J. Borras-Almenar
• 4.26 N-Ferrocenyl Amine and Some Reactive Derivatives p. 333 Max Herberhold and Heidi E. Maisel and Bernd Wrackmeyer
• 4.27 Polyoxomolybdate Clusters: Nanoscopic Wheels and Balls p. 340 Leroy Cronin and Ekkehard Diemann and Achim Muller
• 4.28 One-Pot Preparation of Ru[subscript 3](CO)[subscript 12] from RuCl[subscript 3] - 3 H[subscript 2]O p. 347 Guy Lavigne and Catherine Saccavini and Remi Chauvin
• 4.29 Low Temperature Synthesis of Barium Amides and Phenoxides p. 352 Simon R. Drake and Philip Hall and David J. Otway
• 4.30 Alumazene--Inorganic Benzene Analog p. 357 Jiri Pinkas
• 4.31 Coordination Chemistry of Organic Free Radicals: Synthesis and Magnetic Properties p. 360 A. Alberola and E. Coronado and F. M. Romero
• 4.32 Discovery Research with Arene Chromium Tricarbonyl Chemistry p. 364 Allen D. Hunter
• 4.33 Discovery Research with Cr, Mo, and W Nitrosyl Complexes: A Multi-Step Organometallic Synthesis p. 368 Allen D. Hunter and J. D. Woollins
• Subject Index p. 373